関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 1-Chloro-3-methoxypropane | HCID 118927 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 6-Bromo-2H-1,4-benzoxazin-3(4H)-one | HCID 16218142 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-bromo-4-(3-methoxypropyl)-4H-benzo[1,4]oxazin-3-one | HCID 23148519 | — |
反応手順
The suspension of 9.87 g of 6-bromo-4H-benzo[1,4]oxazin-3-one [24036-52-0], 9.40 g of 1-chloro-3-methoxypropane, potassium fluoride on alumina (Fluka 60244), 0.144 g of potassium iodide in 500 ml of acetonitrile is stirred at 100° C. over 40 hours. The reaction mixture is cooled to room temperature and filtered through Hyflo, and the filtrate is concentrated by evaporation to dryness. The title compound is obtained as a slightly yellowish solid from the residue by crystallization from ethyl acetate. Rf=0.43 (1:1 EtOAc-heptane). Rt=4.27 (gradient I). m.p. 193-195° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07868036B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-658a8b47ad394f8fa6693bdf46507888 |
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| 出典メモ | uspto-grants-2011_01 |
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